Hydrochloric Acid → Dichlorobis[(propan-2-yl)oxy]silane

This material is prepared after the manner of Chappelow et al. (J. Org. Chem. 1960, 25, 435-459.) 2-Propanol (887 g, 14.8 mol) was added slowly over a period of three hours under an atmosphere of Ar to SiCl4 (1475 g, 8.7 mol) at 0° C. The vented HCl gas from the reaction was neutralized by bubbling through a 25% (w/v) solution of KOH in water. The solution was allowed to react for 3 h whereupon, Ar was bubbled through the solution for 30 min. The solution was then distilled through a 30 cm Hemple column packed with 3 mm glass beads (Pot Temp: 180° C., Vapor Temp: 120° C.). The resulting fractions were analyzed by 1H NMR. Fraction A: 411 g (95% Mono: 5% Di); Fraction B: 184 g (22% Mono, 76% Di, 2% Tri); Fraction C: 511 g—27% yield, (95% Di, 5% Tri); and Fraction D: 393 g (50% Di, 50% Tri). Fractions B and D were pooled with other impure cuts from other runs and redistilled at a latter date. 1H NMR (CDCl3, 300 mHz) δ Mono: 4.53 (h, J=6.2 Hz, 1 H), 1.31 (d, J=6.2 Hz, 6 H). Di: 4.41 (h, J=6.2 Hz, 2 H), 1.26 (d, J=6.2 Hz, 12 H); Tri: 4.29 (h, J=6.2 Hz, 3 H), 1.21 (d, J=6.2 Hz, 12 H). 13C NMR (CDCl3, 75.5 mHz) δ Di: 69.27, 24.85.

1. customby bubbling through a 25% (w/v) solution of KOH in water
2. customto react for 3 h whereupon, Ar
3. customwas bubbled through the solution for 30 min
4. distillationThe solution was then distilled through a 30 cm Hemple column
5. custompacked with 3 mm glass beads (Pot Temp: 180° C., Vapor Temp: 120° C.)
6. distillationredistilled at a latter date

ORD record

ord-3f311e632e424dca83b4c21db3967e30

Source dataset

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08759508B2